Abstract: To develop inexpensive and efficient Sb(Ⅴ), As(Ⅴ) removal materials for water bodies, an orthogonal experiment was designed to prepare ferrihydrite /palygorskite composite material (Fh-ACPal), taking calcination temperature, acid concentration, and iron oxide loading as the main influencing factors. The optimal modification method was explored, and the adsorption behavior of Fh-ACPal for As(Ⅴ) and Sb(Ⅴ) in both single and double solute aqueous solutions across varying environmental conditions was investigated. To elucidate its adsorption mechanism, Fh-ACPal was characterized by using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), BET pore structure analysis, X-ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM). The results showed that under the modified conditions of calcination temperature of 350 ℃, hydrochloric acid concentration of 2.0 mol/L, and ferric chloride concentration of 2.0 mol/L, the prepared Fh-ACPal had the best adsorption capacity. When pH was 4 and the dosage of Fh-ACPal was 1 g/L, the maximum monolayer adsorption capacities of Fh-ACPal for As(Ⅴ) and Sb(Ⅴ) were 26.44 and 42.38 mg/g, respectively. In a single solute system, both Freundlich and Langmuir isotherm adsorption models could well fit the process of Fh-ACPal adsorbing Sb(Ⅴ), while the process of Fh-ACPal adsorbing As(Ⅴ) could only fit Freundlich model well. In a dual solute system, Sb(Ⅴ) further formed multi-layered adsorption on As (V) surface that had been preferentially adsorbed by Fh-ACPal. The BET isothermal adsorption model could fit this process well. Based on the experimental and characterization results, it has been proven that the loaded iron oxide is ferrihydrite (Fh), and the modified Fh-ACPal has a specific surface area of 224.84 m²/g. At the same time, most of Sb (Ⅴ) enters the interior of Fh-ACPal crystal through co-precipitation and is stably bound. Most of As(Ⅴ) is mainly adsorbed by Fh-ACPal through surface complexation to form inner spherical complexes. When As (Ⅴ) and Sb (Ⅴ) coexist, the inhabitation of Sb(Ⅴ) adsorption by As(Ⅴ) is mainly due to As(Ⅴ) preferentially occupying the adsorption sites shared by Fh-ACPal surface, which hinders the co-precipitation of Sb(Ⅴ) and Fh-ACPal. The study has demonstrated the effectiveness of ferrihydrite/palygorskite composite materials in removing Sb(Ⅴ) and As(Ⅴ) from water, providing a theoretical reference for the treatment of antimony and arsenic heavy metal pollution in water.